CN114406261B - Sheath die and sheath method for hot isostatic pressing sintering - Google Patents

Sheath die and sheath method for hot isostatic pressing sintering Download PDF

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Publication number
CN114406261B
CN114406261B CN202210045086.4A CN202210045086A CN114406261B CN 114406261 B CN114406261 B CN 114406261B CN 202210045086 A CN202210045086 A CN 202210045086A CN 114406261 B CN114406261 B CN 114406261B
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sheath
gasket
sleeve
die
pressure head
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CN114406261A (en
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王兴安
杨晨
孙旭东
吕卉
刘旭东
惠宇
那兆霖
毕孝国
曾章表
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Dalian University
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Dalian University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • C04B35/645Pressure sintering
    • C04B35/6455Hot isostatic pressing
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/04Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06Details, accessories, or equipment peculiar to furnaces of these types
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • B22F2003/153Hot isostatic pressing apparatus specific to HIP
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27MINDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
    • F27M2003/00Type of treatment of the charge
    • F27M2003/04Sintering

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a sheath die and a sheath method for hot isostatic pressing sintering, and belongs to the technical field of hot isostatic pressing sintering. The sheath die comprises a cylinder structure consisting of a bottom pad and an outer sleeve, an upper pressure head is arranged at the top of the cylinder, and the outer diameter of the upper pressure head is smaller than the inner diameter of the cylinder structure; be equipped with in the barrel structure and wait the sheath sample, wait that the sheath sample is by sheath overcoat sheath, the gasket I centre gripping is passed through at sheath overcoat's both ends, is equipped with the sleeve pressure head on being close to between gasket I of pressure head and the pressure head, is equipped with gasket II, die sleeve and lower sleeve pressure head in proper order from gasket I one side between gasket I and the bottom pad that is close to the bottom pad. The invention realizes the high vacuum in the sheath and the welding of the sheath in one step, has good welding performance of sheath materials, high vacuum degree in the sheath, further improves the success rate of hot isostatic pressing sintering and saves energy.

Description

Sheath die and sheath method for hot isostatic pressing sintering
Technical Field
The invention relates to a sheath die and a sheath method for hot isostatic pressing sintering, and belongs to the technical field of hot isostatic pressing sintering.
Background
Hot isostatic pressing (Hot Isostatic Pressing, HIP) is a process that utilizes high temperature and high pressure loading (typically gas) to effect the preparation of powder or bulk material and the formation of parts. The outstanding advantage is that the gas is passed through an inert gas such as Ar, N in a device with excellent tightness 2 The green body is uniformly extruded from all directions by the pressure transmission medium, and the air holes of all parts are well driven and filled, so that the aim of almost completely densification is fulfilled.
The hot isostatic pressing sintering is mainly applied to densification sintering of powder and blocks, and because of the special pressurizing mode, the powder needs to be subjected to cladding treatment before sintering, and the powder needs to be subjected to cladding if samples are required to be subjected to diffusion connection. If gaps exist in the sheath, the problems that powder leaks and gas goes deep into the sheath and cannot reach the target pressure occur in the sintering process; if the sheath is too thick and complicated, part of air pressure is born by the sheath in the pressing process, and the pressure applied on the sample can be far less than the set pressure; if a high vacuum is not achieved in the envelope, this also results in a barrier to the application of pressure. The problems cannot be accurately checked before the hot isostatic pressing sintering, and finally the failure of the hot isostatic pressing sintering is caused, so that the selection of proper sheathing materials and sheathing methods is the key of the work before the hot isostatic pressing sintering.
The sheath material used in the hot isostatic pressing process needs to have good high temperature resistance, excellent weldability and high plasticity. The currently used sheathing materials are mainly glass (e.g., pyrex glass, quartz glass, vycor glass, etc.) and metal (e.g., ti, ni, mo, W, stainless steel, etc.). For ceramic materials, the glass sheath has the problem that the softening temperature is not matched with the ceramic sintering temperature, so that the application of the glass sheath in the ceramic hot isostatic pressing sintering process is limited. At present, a metal sheath is usually finished by adopting a mechanical processing and welding mode, and vacuumizing and welding are carried out step by step, so that the high vacuum degree in the sheath cannot be ensured, and the problems of complex manufacturing process, multiple welding seams and low welding success rate are also solved. The presence of a weld during the hot isostatic pressing sintering process can hinder densification of the material, both of which can ultimately lead to failure of the material to form and densify.
Disclosure of Invention
The purpose of the invention is that:
1) A high vacuum, low weld sheath die for hot isostatic pressing sintering is provided.
2) The method for covering the steel wire rod with the high vacuum degree can achieve the high vacuum degree in one step, has few welding seams, remarkably reduces the welding seams, and greatly improves the quality and success rate of covering.
In order to achieve the above object, the present invention provides the following technical solutions:
a high-vacuum sheath die with few welding lines for hot isostatic pressing sintering and a sheath method thereof are provided, wherein the sheath of a material to be sintered is realized by hot pressing sintering once.
The invention provides a sheath die for hot isostatic pressing sintering, which comprises a cylinder structure consisting of a bottom pad and an outer sleeve, wherein an upper pressure head is arranged at the top of the cylinder, and the outer diameter of the upper pressure head is smaller than the inner diameter of the cylinder structure; the cylinder structure is internally provided with a sample to be wrapped, the sample to be wrapped is wrapped by a wrapping sleeve, two ends of the wrapping sleeve are clamped by a gasket I, an upper sleeve pressure head is arranged between the gasket I close to the upper pressure head and the upper pressure head, and a gasket II, a die sleeve and a lower sleeve pressure head are sequentially arranged between the gasket I close to the bottom pad and the bottom pad from one side of the gasket I; the die sleeve is of a convex structure, the protruding part is arranged between the gasket II and the lower sleeve pressure head, and the other two ends of the protruding part are respectively clamped on the side face of the lower sleeve pressure head and the side face of the gasket I close to the upper pressure head, so that the gasket I, the sheath jacket and the gasket II are fixed in position.
Further, in the above technical scheme, the cylinder structure formed by the bottom pad and the outer sleeve is a hollow cylinder without a cover or a cube.
Further, in the above technical solution, the size of the gasket i is equal to or greater than the diameter of the upper sleeve ram; the length of the gasket II is the same as that of the sheath jacket, and two ends of the gasket II support the gasket I.
Further, in the above technical scheme, the diameter of the gasket I is 50 mm-220 mm, and the thickness is 0.1-0.5 mm.
Further, in the above technical scheme, the sample to be sheathed comprises ceramics, metal powder or blocks, the shape is any shape, the size is 5 mm-80 mm, and the thickness is 1-30 mm; and the melting point of the sample to be sheathed is higher than the sintering temperature of the hot isostatic pressing.
Further, in the above technical solution, the material of the sheath mold is high-strength graphite or conductive graphite; all the contact surfaces among all the parts in the sheathing die are detachably connected, and graphite paper is padded.
The invention also provides a sheathing method of the sheathing mold for hot isostatic pressing sintering, which comprises the following steps:
1) Material preparation and sheath manufacturing:
cleaning the surface of a sample to be sheathed; preparing a sheath jacket material with a melting point higher than the sintering temperature of hot isostatic pressing, and cleaning the surface of the sheath jacket material;
2) Combination of the mold:
combining a sheathing die, and putting a sample to be sheathed and a sheathing jacket;
3) Hot pressing and sintering:
placing the whole set of sheath die obtained by the combination of the step 2) into a furnace chamber of a hot-press sintering furnace, vacuumizing the furnace chamber, hot-press sintering according to the set temperature, pressure and time, and welding and forming; and taking out the sample after the sheathing die and the sample are cooled to room temperature, and using the obtained sample for hot isostatic pressing sintering.
In the technical scheme, the cleaning agent used in the step 1) comprises ethanol or acetone, and the oil stain and dust on the surfaces of the sample to be sheathed and the sheath material are removed by an ultrasonic cleaning method.
Further, in the above technical solution, the step 3) of evacuating the cavity includes: firstly, a mechanical pump and a pre-pumping valve are used for vacuumizing the furnace chamber to be less than 10Pa, and then a diffusion pump is opened for vacuumizing the furnace chamber to be 1 multiplied by 10 -3 Pa or less, remain trueAnd (5) hollowness.
Further, in the technical scheme, the temperature of hot-pressing sintering in the step 3) is 600-1500 ℃, the pressure is 20-50 MPa, and the heat preservation and pressure maintaining time is 0.5-3 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention realizes the high vacuum in the sheath and the welding of the sheath in one step: simultaneously vacuuming to 1X 10 in the sintering process by hot pressing -3 And the pressure is lower than Pa, so that welding of the sheath material is realized, and high vacuum in the sheath is realized. The method has the characteristics of high sintering speed, good welding performance of the sheath material, high vacuum degree in the sheath, further improvement of the success rate of hot isostatic pressing sintering, energy conservation and the like. Realize the one-time preparation of the sheath with high vacuum degree and less welding lines. Solves the problems of difficult preparation and high cost of the existing hot isostatic pressing sintering sheath die.
2. The prepared sheath has no requirement on the shape and the material of the material to be sheathed, and can solve the problem of difficult sheath of special-shaped materials and the like.
3. The sheath prepared by the invention has small raw material consumption and thickness of only 0.1-0.5 mm, can ensure that the pressure is uniformly and nondestructively applied to the surface of a sample in the hot isostatic pressing sintering process, and can save a great amount of cost. And the smaller thickness of the sheath material and the method for realizing welding through hot-pressing sintering greatly improve the success rate of the sheath, further improve the success rate of hot isostatic pressing sintering and save the cost.
Drawings
Fig. 1 is a schematic diagram of a capsule mold for hot isostatic pressing sintering according to the present invention.
In the figure, 1, an upper pressure head; 2. an upper sleeve pressure head; 3. a gasket I; 4. a lower sleeve pressure head; 5. a bottom pad; 6. a jacket; 7. a sample to be sheathed; 8. a jacket sleeve; 9. a gasket II; 10. and (5) die sleeve.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
The invention is further illustrated by the following figures and examples.
As shown in fig. 1, a sheath die for hot isostatic pressing sintering comprises a cylinder structure consisting of a bottom pad 5 and an outer sleeve 6, wherein an upper pressure head 1 is arranged at the top of the cylinder, and the outer diameter of the upper pressure head 1 is smaller than the inner diameter of the cylinder structure; the cylinder structure is internally provided with a sample 7 to be sleeved, the sample 7 to be sleeved is sleeved by a sleeve jacket 8, two ends of the sleeve jacket 8 are clamped by a gasket I3, an upper sleeve pressure head 2 is arranged between the gasket I3 close to the upper pressure head 1 and the upper pressure head 1, and a gasket II 9, a die sleeve 10 and a lower sleeve pressure head 4 are sequentially arranged between the gasket I3 close to a bottom pad 5 and the bottom pad 5 from one side of the gasket I3; the die sleeve 10 is of a convex structure, the protruding part is arranged between the gasket II 9 and the lower sleeve pressure head 4, and the other two ends of the protruding part are respectively clamped on the side face of the lower sleeve pressure head 4 and the side face of the gasket I3 close to the upper pressure head 1, so that the gasket I3, the sleeve jacket 8 and the gasket II 9 are fixed in position.
The cylinder structure formed by the bottom pad 5 and the outer sleeve 6 is a hollow cylinder without a cover or a cube.
The size of the gasket I3 is equal to or larger than the diameter of the upper sleeve pressure head 2; the length of the gasket II 9 is the same as that of the jacket 8, and two ends of the gasket II 9 support the gasket I3.
The diameter of the gasket I3 is 50 mm-220 mm, and the thickness is 0.1-0.5 mm.
The sample 7 to be sheathed comprises ceramics, metal powder or blocks, the shape is any shape, the size is 5 mm-80 mm, and the thickness is 1-30 mm; the melting point of the sample 7 to be sheathed is higher than the sintering temperature of the hot isostatic pressing.
The material of the sheathing die is high-strength graphite or conductive graphite; all the contact surfaces among all the parts in the sheathing die are detachably connected, and graphite paper is padded.
Example 2
A capsule method for a capsule mould for hot isostatic pressing sintering, comprising the steps of:
1) Material preparation and sheath manufacturing:
cleaning the surface of a sample to be sheathed; preparing a sheath jacket material with a melting point higher than the sintering temperature of hot isostatic pressing, and cleaning the surface of the sheath jacket material;
2) Combination of the mold:
combining a sheathing die, and putting a sample to be sheathed and a sheathing jacket;
3) Hot pressing and sintering:
placing the whole set of sheath die obtained by the combination of the step 2) into a furnace chamber of a hot-press sintering furnace, vacuumizing the furnace chamber, hot-press sintering according to the set temperature, pressure and time, and welding and forming; and taking out the sample after the sheathing die and the sample are cooled to room temperature, and using the obtained sample for hot isostatic pressing sintering.
The cleaning agent used in the step 1) comprises ethanol or acetone, and the oil stain and dust on the surfaces of the samples to be sheathed and the sheath materials are removed by an ultrasonic cleaning method.
The step 3) of vacuumizing the furnace chamber comprises the following steps: firstly, a mechanical pump and a pre-pumping valve are used for vacuumizing the furnace chamber to be less than 10Pa, and then a diffusion pump is opened for vacuumizing the furnace chamber to be 1 multiplied by 10 -3 Pa or less, and maintaining the vacuum degree.
The temperature of hot pressing sintering in the step 3) is 600-1500 ℃, the pressure is 20-50 MPa, and the heat preservation and pressure maintaining time is 0.5-3 h.
Example 3
A sheath mould and sheath for hot isostatic pressing sintering of boron carbide ceramics with high vacuum degree and less welding lines. The specific steps of this embodiment are as follows:
1) Material to be covered and material for covering
The material to be sheathed is boron carbide (B) 4 C) The material of the block body and the sheath jacket is TA1:
TA1 diameter 120mm, thickness 0.15mm.
2) Sheath die assembly constitution
And (3) an upper pressure head: the material is high-strength graphite, the diameter is 140mm, and the height is 60mm;
upper sleeve pressure head: the material is high-strength graphite, the outer diameter is 120mm, the inner diameter is 105mm, and the height is 80mm;
gasket I: the material is high-strength graphite, the outer diameter is 120mm, the inner diameter is 90mm, and the height is 10mm;
the lower sleeve pressure head: the material is high-strength graphite, the outer diameter is 120mm, the inner diameter is 105mm, and the height is 80mm;
a base cushion: the material is high-strength graphite, the diameter is 185mm, and the height is 50mm;
an outer sleeve: the material is electrode graphite, the outer diameter is 185mm, the inner diameter is 145mm, and the height is 225mm;
gasket II: the material is high-strength graphite, the diameter is 120mm, and the height is 10mm;
die sleeve: the material is high-strength graphite, the outer diameter is 140mm, the inner diameter is 120mm, and the height is 66mm.
3) Manufacturing steps of the sheath
Step one: after TA1 is cut into a size which accords with the die, the surface of TA1 is polished to a metallic color by 120-mesh and 240-mesh sand paper so as to remove the surface oxide film. Then dipping the absorbent cotton into acetone to wipe the surface, washing with deionized water, dipping the absorbent cotton into absolute ethyl alcohol to wipe the surface, and drying at 50 ℃ for 30min to remove dust and greasy dirt on the surface.
Step two: the sequence of the combined die is as follows: the method comprises the steps of a bottom pad, a lower sleeve pressing head 4, a die sleeve 10, a gasket II 9, a gasket I3, a sheath jacket 8, a sample to be sheath 7, a gasket I3, an upper sleeve pressing head 2, an upper pressing head 1 and a sheath 6, wherein all contact surfaces are padded with graphite paper in the combination process.
Step three: the whole set of sheath mould is arranged in a furnace chamber of a hot-press sintering furnace, a diffusion pump is opened after the vacuum degree in the furnace chamber is pumped to below 10Pa through a mechanical pump and pre-pumping valve, and the furnace chamber is pumped to 1 multiplied by 10 -3 Pa or below.
Step four: hot-pressing sintering is carried out, wherein the sintering process comprises the following steps: heating to 800 deg.C for 40min, heating to 6MPa, maintaining the temperature and pressure for 30min while maintaining the vacuum degree in the furnace chamber higher than 1×10 -3 Pa。
Step six: and (5) cooling to room temperature along with a furnace after sintering, and taking out the sheath die to obtain the sheath with high vacuum degree and no weld joint.

Claims (10)

1. A capsule mould for hot isostatic pressing sintering, characterized in that: the sheath die comprises a barrel structure consisting of a bottom pad (5) and an outer sleeve (6), an upper pressure head (1) is arranged at the top of the barrel, and the outer diameter of the upper pressure head (1) is smaller than the inner diameter of the barrel structure; the cylinder structure is internally provided with a sample (7) to be wrapped, the sample (7) to be wrapped is wrapped by a wrapping sleeve (8), two ends of the wrapping sleeve (8) are clamped by a gasket I (3), an upper sleeve pressure head (2) is arranged between the gasket I (3) close to an upper pressure head (1) and the upper pressure head (1), and a gasket II (9), a die sleeve (10) and a lower sleeve pressure head (4) are sequentially arranged between the gasket I (3) close to a bottom pad (5) and the bottom pad (5) from one side of the gasket I (3); the die sleeve (10) is of a convex structure, the protruding part is arranged between the gasket II (9) and the lower sleeve pressing head (4), and the other two ends of the protruding part are respectively clamped on the side face of the lower sleeve pressing head (4) and the side face of the gasket I (3) close to the upper pressing head (1), so that the positions of the gasket I (3), the jacket sleeve (8) and the gasket II (9) are fixed.
2. The capsule mould according to claim 1, wherein: the cylinder structure formed by the bottom pad (5) and the outer sleeve (6) is a hollow cylinder without a cover or a cube.
3. The capsule mould according to claim 1, wherein: the size of the gasket I (3) is equal to or larger than the diameter of the upper sleeve pressure head (2); the length of the gasket II (9) is the same as that of the sheath jacket (8), and two ends of the gasket II (9) support the gasket I (3).
4. A capsule mould according to claim 3, wherein: the diameter of the gasket I (3) is 50-220 mm, and the thickness is 0.1-0.5 mm.
5. The capsule mould according to claim 1, wherein: the sample (7) to be sheathed comprises ceramics, metal powder or blocks, the shape is any shape, the size is 5 mm-80 mm, and the thickness is 1-30 mm; the melting point of the sample (7) to be sheathed is higher than the sintering temperature of the hot isostatic pressing.
6. The capsule mould according to claim 1, wherein: the material of the sheathing die is high-strength graphite or conductive graphite; all the contact surfaces among all the parts in the sheathing die are detachably connected, and graphite paper is padded.
7. A sheathing method of a sheathing mold according to any one of claims 1 to 6, wherein: the method comprises the following steps:
1) Material preparation and sheath manufacturing:
cleaning the surface of a sample to be sheathed; preparing a sheath jacket material with a melting point higher than the sintering temperature of hot isostatic pressing, and cleaning the surface of the sheath jacket material;
2) Combination of the mold:
combining a sheathing die, and putting a sample to be sheathed and a sheathing jacket;
3) Hot pressing and sintering:
placing the whole set of sheath die obtained by the combination of the step 2) into a furnace chamber of a hot-press sintering furnace, vacuumizing the furnace chamber, hot-press sintering according to the set temperature, pressure and time, and welding and forming; and taking out the sample after the sheathing die and the sample are cooled to room temperature, and using the obtained sample for hot isostatic pressing sintering.
8. The sheathing method according to claim 7, wherein: the cleaning agent used in the step 1) comprises ethanol or acetone, and the oil stain and dust on the surfaces of the samples to be sheathed and the sheath materials are removed by an ultrasonic cleaning method.
9. The sheathing method according to claim 7, wherein: the step 3) of vacuumizing the furnace chamber comprises the following steps: firstly, a mechanical pump and a pre-pumping valve are used for vacuumizing the furnace chamber to be less than 10Pa, and then a diffusion pump is opened for vacuumizing the furnace chamber to be 1 multiplied by 10 -3 Pa or less, and maintaining the vacuum degree.
10. The sheathing method according to claim 7, wherein: the temperature of hot pressing sintering in the step 3) is 600-1500 ℃, the pressure is 20-50 MPa, and the heat preservation and pressure maintaining time is 0.5-3 h.
CN202210045086.4A 2022-01-14 2022-01-14 Sheath die and sheath method for hot isostatic pressing sintering Active CN114406261B (en)

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